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Yellow copper ore, pyrite is typical of sulfide ore minerals, they are typically referred to as a job separator copper sulfur separation. In the separation of copper and sulfur, the flotation method is of great significance, and the research of inhibitors in flotation is a very important direction. The traditional copper-sulfur flotation separation method is to add a large amount of lime to the slurry and carry out sulfur-inhibiting float copper in a high alkalinity environment. The process is quite mature and the separation effect is good, but there is also easy scaling in the use process. Consolidation, blockage of pipelines, corrosion of equipment, and serious pollution of mine wastewater are not conducive to the contradiction of comprehensive recovery of valuable associated components. Therefore, it is of great theoretical and practical significance to research and develop high-efficiency pyrite inhibitors to achieve lime-free copper-sulfur flotation separation under low-alkali know-how and to improve the comprehensive utilization of mineral resources.
I. Single mineral test study
(1) Preparation of single mineral ore sample
The pyrite (FeS 2 ) used in the test was taken from a mine ore. The pyrite is crushed, selected, and porcelain ball milled to below 100 mesh, and then sieved to remove fine ore particles with a 250-mesh sieve, and the obtained mineral of 100-250 mesh size is used as a test sample, and stored in a vacuum dryer. spare. The purity of pyrite was 95.74%, and the chemical analysis results of the main elements are shown in Table 1.
Table 1 Chemical analysis results of main elements of pyrite
element
Cu
Fe
S
content
0.47
44.8
51.03
The chalcopyrite (CuFeS 2 ) used in the test was taken from the chalcopyrite flotation concentrate of Dexing Copper Mine. After degreasing, the drug was removed and sieved to remove -250 mesh fine ore. The obtained ore sample was used as a test. Samples were stored in a vacuum desiccator for later use. The purity of chalcopyrite was 99.05% after analysis. The main elemental composition analysis results are shown in Table 2.
Table 2 Chemical analysis results of main elements of chalcopyrite %
element
Cu
Fe
S
content
34.45
30.35
34.80
(II) Effect of calcium hypochlorite on the floatability of pyrite and chalcopyrite
Calcium hypochlorite [Ca (ClO) 2], dissolved in water and release oxygen while simultaneously decomposing and Ca 2 +, has a strong oxidation resistance, when the solution has at pH <9, Ca 2 + in the aqueous solution hardly occurs Hydrolysis, mainly in the form of ions, in view of this, the effect of the amount of Ca(ClO) 2 on the right float of chalcopyrite and pyrite was tested. The test conditions and results are shown in Fig. 1.
It can be seen from Fig. 1 that Ca(ClO) 2 does not change the floatability of chalcopyrite when the pH of the slurry is 7-8, but it has a good inhibitory effect on pyrite. With the increase of its dosage, the floating rate of pyrite is greatly reduced. When the dosage is 1000g/t, the recovery rate of pyrite is only 19.20%. When the dosage continues to increase, the recovery rate does not change much.
(III) Flotation separation test of artificial mixed ore
According to the previous single mineral test, in the low alkalinity environment of pH=7-8, Ca(ClO) 2 showed good inhibition performance to pyrite, but did not change the floatability of chalcopyrite. In order to further study the inhibitory effect of Ca(ClO) 2 on pyrite and the possibility of copper and sulfur separation, the experimental study on the separation of artificial mixed ore by different copper-sulfur ratio was carried out under low alkali conditions. The pH of the slurry was adjusted to 7-8 with NaOH, the amount of Dinghuang was 60 g/t, the amount of Ca(ClO) 2 was 1000 g/t, and the amount of 2 # oil was 90 g/t. The test results are shown in Table 3.
Table 3 Flotation separation results of chalcopyrite and pyrite mixed ore
Test number
product name
Yield
Copper grade
Sulfur grade
Copper recovery
Sulfur recovery
Chalcopyrite
Pyrite
1:1
Concentrate
Tailings
54.49
46.51
30.20
1.83
38.60
47.60
95.07
4.93
48.72
51.28
Chalcopyrite
Pyrite
1:5
Concentrate
Tailings
24.92
75.08
22.28
0.77
44.18
49.71
90.60
9.40
22.78
77.22
Chalcopyrite
Pyrite
1:10
Concentrate
Tailings
16.22
83.78
19.47
0.48
46.19
50.20
88.72
11.28
15.12
84.88
Chalcopyrite
Pyrite
1:20
Concentrate
Tailings
10.37
89.63
18.35
0.21
46.19
50.73
91.04
8.96
9.53
90.47
It can be seen from Table 3 that Ca(ClO) 2 has good inhibitory properties on pyrite and is highly adaptable. Under the low alkali conditions of pulp pH=7-8, Ca(ClO) 2 is used as an inhibitor of pyrite. It can realize the separation of copper and sulfur flotation and obtain better separation index.
2. Analysis of inhibition mechanism of Ca(ClO) 2 on pyrite
According to the basic theory of mineral flotation, the main way for inhibitors to inhibit minerals is to eliminate the activated film or collector film on the mineral surface, and form a hydrophilic film on the mineral surface. In order to further understand the role of Ca(ClO) 2 in the separation of copper and sulfur, better guide the separation process of copper and sulfur, through the surface chemical reaction and Raman spectroscopy analysis, the Ca(ClO) in the separation process of low alkalinity copper and sulfur was studied. 2 inhibition mechanism of pyrite.
(I) Effect of Ca(ClO) 2 on the chemical composition of pyrite mineral surface
Studies have shown that under alkaline or neutral conditions, the oxidation of (1) to (3) may occur on the surface of pyrite, and they have also detailed the properties and effects of elemental sulfur on the surface of sulfide minerals. It is considered that the zero-valent sulfur (S 0 ) on the surface of the sulfide ore is a very unstable substance, and under oxidation conditions, it is oxidized to S 2 O 3 2 - , SO 4 2 - , HSO 4 2 - .
FeS 2 +2H 2 O→Fe(OH) 2 +S0+2H + +ne, (1)
FeS 2 +5H 2 O→Fe(OH) 2 +S 2 0 3 2 - +8H + +6e, (2)
FeS 2 +10H 2 O→Fe(OH) 2 +2S0 4 2 - +18H + +14e, (3)
2S 0 +3H 2 O→S 2 0 3 2 - +6H + +4e, (4)
S 0 +4H 2 O→S0 4 2 - +8H + +6e, (5)
S 0 +4H 2 O→HS0 4 2 - +7H + +6e, (6)
Ca (ClO) 2 is a strong oxidant, adding a small amount of Ca (ClO) 2 in the floating mineral slurry, the slurry was able to make a strong oxidizing atmosphere. At this time, in addition to the oxidation reaction shown in (1) to (6), the surface of the pyrite may be further oxidized to S 2 O 3 2 - , SO 4 2 - , HSO 4 2 - In addition, it is more important that a large amount of Fe(OH) 2 formed by its surface reaction is further oxidized by Fe(OH) 3 as shown in the formula (7). Fe(OH) 3 is a slightly water-soluble compound, and its solubility product Ksp is much smaller than Fe(OH) 2 , and it can be stably present in an alkaline medium. Therefore, it is possible to determine a large amount of Fe(OH) 3 produced on the surface of pyrite, which is a major cause of inhibition of pyrite.
2Fe(OH) 2 +ClO - +H 2 O=2Fe(OH) 3 ↓+Cl - (7)
On the other hand, Ca (ClO) 2 was dissolved in a large amount of water will be ionized Ca 2 +, studies have shown that, when the solution pH at 9, Ca 2 + difficult to hydrolyze <in aqueous solution, is present in substantially ionic form. Accordingly, the Ca 2 + will be generated by the oxidation of pyrite SO 4 2 - binding a precipitate. In addition, the slurry will absorb part of the CO 2 during the flotation aeration process, producing a certain amount of CO 3 2 - , since K sp calcium carbonate <K sp calcium sulfate <K sp calcium hydroxide <K sp calcium chloride <, then In the aqueous solution, the reactions shown in the formulas (8), (9), and (10) occur, and finally the calcium component of the mineral surface is mainly CaCO 3 which is chemically stable under alkaline conditions, and its solubility product. Ksp is only 2.8×10 -9 , which is a slightly soluble compound and is firmly wrapped on the surface of pyrite. Therefore, it is considered to be another cause of the deterioration of the floatability of pyrite.
CaSO 4 +CO 3 2 - =CaCO 3 ↓+SO 4 2 - (8)
Ca(OH) 2 +CO 2 =CaCO 3 ↓+H 2 O (9)
CaCl 2 +CO 3 2 - =CaCO 3 ↓+2Cl - (10)
Through the above series of chemical reaction analysis, it can be considered that the inorganic oxidant Ca(ClO) 2 inhibits pyrite, and the mechanism for achieving low alkalinity and no lime, copper and sulfur separation is low alkalinity without lime and copper in slurry pH=7-8. The mechanism of separation is that under the low alkali condition of slurry pH=7-8, Ca(ClO) 2 oxidizes the surface to produce a large amount of Fe(OH) 3 hydrophilic substance; on the other hand, Ca(ClO) 2 in most aqueous ionized Ca 2 + ions in the solution and CO 3 2 - binding, combined with the product adsorbed on the pyrite surface stabilized, so that Fe (OH) 3 and CaCO 3 act synergistically in the pyrite surface, resulting in The surface of the pyrite forms a hydrophilic film with main components of Fe(OH) 3 and CaCO 3 , which greatly enhances the hydrophilicity of the surface of the pyrite, so that it is inhibited in the pulp and achieves the separation of lime-free copper and sulfur.
(2) Raman spectroscopy analysis of pyrite mineral surface
In order to further clarify the inhibition mechanism of Ca(ClO) 2 on pyrite, the existence of the above series of chemical reactions on the surface of pyrite minerals was confirmed. The Raman spectra of the pyrite mineral surface before and after Ca(ClO) 2 treatment were studied under low alkali conditions with slurry pH=7-8. Fig. 2(a) is a Raman spectrum of the mineral surface of the pyrite after soaking with the xanthate solution; Fig. 2(b) is the soaking of the pyrite by the xanthate solution, and then soaked by the Ca(ClO) 2 solution The final mineral surface Raman spectrum after the action.
Fig. 2 Raman spectrum of the surface of pyrite mineral before and after Ca(ClO) 2
It can be seen from Fig. 2(a) that under the low alkali condition of slurry pH=7-8, the Raman spectrum of the pyrite surface after the action of xanthate shows peaks only at 343 cm -1 and 379 cm -1 , and the two The peak values ​​are caused by pyrite Fe-[S 2 ] stretching vibration. Therefore, it can be inferred that Dinghuang is difficult to chemically react on the surface of pyrite. (B) 2 shows that, after the addition of Ca (ClO) 2, pyrite undergone significant changes, in addition to the Raman spectrum 343cm -1, 379cm -1 near the pyrite occur Fe- [S In addition to the two stretching vibration peaks of 2 ], there is another peak near 282 cm -1 , which is a typical CaCO 3 active peak, and no other vibration peaks appear. Therefore, it can be explained that under the low alkali condition of slurry pH=7-8, after the surface of pyrite is treated by Ca(ClO) 2 solution, a hydrophilic film of CaCO 3 is newly formed, so that it is Sufficiently suppressed.
Third, the conclusion
(1) Single mineral flotation test shows that Ca(ClO) 2 does not affect the floatability of chalcopyrite under the condition of low pH of 7-8, and shows good inhibition performance to pyrite.
(2) The flotation separation test of artificial mixed ore shows that Ca(ClO) 2 has good selectivity in the process of copper-sulfur flotation separation under the low alkali environment of slurry pH=7-8, and the adaptability is strong. Successfully realized the separation of lime-free copper-sulfur flotation of artificial mixed ore with various copper-sulfur ratios, and obtained better indicators.
(3) Mineral surface chemical reaction and Raman spectroscopy analysis show that under low alkalinity conditions, Ca(ClO) 2 oxidizes the surface of pyrite, and the surface is mainly composed of Fe(OH) 3 and CaCO 3 . The film improves the hydrophilicity of the mineral surface of pyrite, so that it is sufficiently suppressed in the copper-sulfur flotation separation operation, thereby successfully achieving the separation of lime-free copper and sulfur.